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Dimethylformamide → 4-[1-Benzyl-4-(3-methoxy-phenyl)-piperidin-4-yl]-benzonitrile

HRID 2085460
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HRID 2085460 반응식
[CH2:1]([N:8]1[CH2:13][CH2:12][C:11]([C:22]2[CH:27]=[CH:26][C:25](OS(C(F)(F)F)(=O)=O)=[CH:24][CH:23]=2)([C:14]2[CH:19]=[CH:18][CH:17]=[C:16]([O:20][CH3:21])[CH:15]=2)[CH2:10][CH2:9]1)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.[CH3:36][N:37](C=O)C>C(OCC)C.[C-]#N.[Zn+2].[C-]#N>[CH2:1]([N:8]1[CH2:13][CH2:12][C:11]([C:22]2[CH:27]=[CH:26][C:25]([C:36]#[N:37])=[CH:24][CH:23]=2)([C:14]2[CH:19]=[CH:18][CH:17]=[C:16]([O:20][CH3:21])[CH:15]=2)[CH2:10][CH2:9]1)[C:2]1[CH:3]=[CH:4][CH:5]=[CH:6][CH:7]=1
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참가 물질

5

반응물 2

HCID 6228DimethylformamideHCID 54436264Trifluoro-methanesulfonic acid 4-[1-benzyl-4-(3-methoxy-phenyl)piperidin-4-yl]-phenyl ester

생성물 1

HCID 227299114-[1-Benzyl-4-(3-methoxy-phenyl)-piperidin-4-yl]-benzonitrile수율 92%

시약·촉매·용매 2

HCID 11186Zinc cyanide (Zn(CN)2)촉매HCID 3283Diethyl Ether용매

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온도
90 °C

실험 절차

To a solution of trifluoro-methanesulfonic acid 4-[1-benzyl-4-(3-methoxy-phenyl)-piperidin-4-yl]-phenyl ester (2.2 g, 4.34 mmol) in DMF (8 mL) was added zinc cyanide (0.61 g, 5.22 mmol) and tetrakis triphenylphosphine palladium (0.7 g, 0.63 mmol). The reaction was stirred under a nitrogen atmosphere at 90° C. for 5 hours. The mixture was cooled to room temperature and it was diluted with diethyl ether (100 mL). The organic layer was washed with brine (5×10 mL), dried (MgSO4) and concentrated. Purification with hexanes/EtOAc (2:1) afforded 1.52 g (92% yield) of 4-[1-Benzyl-4-(3-methoxy-phenyl)-piperidin-4-yl]-benzonitrile. 1HNMR (400 MHz, CDCl3) δ 7.51 (d, 2H), 7.34 (d, 2H), 7.28-7.18 (comp, 6H), 6.80 (d, 1H), 6.77 (s, 1H), 6.70(d, 1H), 3.75 (s, 3H), 3.39 (s, 2H), 2.63-2.39 (comp, 8H); MS (M+1) 383.2.

후처리

  1. temperatureThe mixture was cooled to room temperature
  2. washThe organic layer was washed with brine (5×10 mL)
  3. dry with materialdried (MgSO4)
  4. concentrationconcentrated
  5. customPurification with hexanes/EtOAc (2:1)

출처 및 근거

ORD 기록
ord-c5c4f273b6c0477fa963dad9433fc13f
출처 데이터셋
uspto-grants-2004_04
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06720336B2

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